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ARTICLE 24
LIQUID PENETRANT STANDARDS
SD-129
421
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ARTICLE 24, SD-129 2007 SECTION V
quantitative recovery of the liquids from the bomb may stable and representative of the samples of interest. These
be achieved readily. The inner surface of the bomb may QC samples can be used to check the validity of the testing
be made of stainless steel or any other material that will process as described in Section 11.
not be affected by the combustion process or products.
Materials used in the bomb assembly, such as the head
gasket and lead-wire insulation, shall be resistant to heat 6. Procedure
and chemical action, and shall not undergo any reaction 6.1 Preparation of Bomb and Sample — Cut a piece of
that will affect the sulfur content of the liquid in the bomb. firing wire 100 mm in length. Coil the middle section
(about 20 mm) and attach the free ends to the terminals.
4.2 Sample Cup, platinum, 24 mm in outside diameter Arrange the coil so that it will be above and to one side
at the bottom, 27 mm in outside diameter at the top, 12 of the sample cup. Insert between two loops of the coil a
mm in height outside, and weighing 10 to 11 g. wisp of cotton or nylon thread of such length that one end
4.3 Firing Wire, platinum, No. 26 B & S gage, 0.41 will extend into the sample cup. Place about 5 mL of
mm (16 thou), 27 SWG, or equivalent. (Warning — The Na2CO3 solution in the bomb (Note 2) and rotate the bomb
switch in the ignition circuit shall be of a type which in such a manner that the interior surface is moistened by
remains open, except when held in closed position by the the solution. Introduce into the sample cup the quantities
operator.) of sample and white oil (Note 3 and Note 4) specified in
4.4 Ignition Circuit, capable of supplying sufficient cur- the following table, weighing the sample to the nearest 0.2
rent to ignite the cotton wicking or nylon thread without mg (when white oil is used, stir the mixture with a short
melting the wire. The current shall be drawn from a step- length of quartz rod and allow the rod to remain in the
down transformer or from a suitable battery. sample cup during the combustion).
4.5 Cotton Wicking or Nylon Sewing Thread, white. NOTE 2 — After repeated use of the bomb for sulfur determinations, a
film may be noticed on the inner surface. This dullness can be removed
by periodic polishing of the bomb. A satisfactory method for doing this
5. Reagents and Materials is to rotate the bomb in a lathe at about 300 rpm and polish the inside
5.1 Purity of Reagents — Reagent grade chemicals shall surface with emery polishing papers Grit No. 2/0, or equivalent paper,
coated with a light machine oil to prevent cutting, and then with a paste
be used in all tests. Unless otherwise indicated, it is
of grit-free chromic oxide and water. This procedure will remove all but
intended that all reagents shall conform to the specifications very deep pits and put a high polish on the surface. Before the bomb is
of the Committee on Analytical Reagents of the American used it shall be washed with soap and water to remove oil or paste left
Chemical Society, where such specifications are available. from the polishing operation.
Other grades may be used, provided it is first ascertained 6.1.1 Warning — Do not use more than 1.0 g total
that the reagent is of sufficiently high purity to permit its of sample and white oil or other low sulfur combustible
use without lessening the accuracy of the determination. material or more than 0.8 g if the IP 12 bomb is used.
5.2 Purity of Water — Unless otherwise indicated, refer- Weight of Weight of
ences to water shall mean water as defined by Type II or Sulfur Content, % Sample, g White Oil, g
III of Specification D 1193. 5 or under 0.6 to 0.8 0.0
Over 5 0.3 to 0.4 0.3
5.3 Barium Chloride Solution (85 g/litre) — Dissolve to 0.4
100 g of barium chloride dihydrate (BaCl2 W 2H2O) in
distilled water and dilute to 1 liter. NOTE 3 — Use of sample weights containing over 20 mg of chlorine
may cause corrosion of the bomb. To avoid this, it is recommended that
5.4 Bromine Water (saturated).
for samples containing over 2% chlorine, the sample weight be based on
5.5 Hydrochloric Acid (sp gr 1.19) — Concentrated the chlorine content as given in the following table:
hydrochloric acid (HCl). Weight of Weight of
Chlorine Content, % Sample, g White Oil, g
5.6 Oxygen, free of combustible material and sulfur
compounds, available at a pressure of 41 kgf/cm2 (40 atm). 2 to 5 0.4 0.4
Over 5 to 10 0.2 0.6
5.7 Sodium Carbonate Solution (50 g/litre) — Dissolve Over 10 to 20 0.1 0.7
135 g of sodium carbonate decahydrate (Na2CO3 W 10H2O) Over 20 to 50 0.05 0.7
or its equivalent weight in distilled water and dilute to
1 litre. NOTE 4 — If the sample is not readily miscible with white oil, some
other low sulfur combustible diluent may be substituted. However, the
5.8 White Oil, USP, or Liquid Paraffin, BP, or equiv- combined weight of sample and nonvolatile diluent shall not exceed 1.0
alent. g or more than 0.8 g if the IP 12 bomb is used.
5.9 Quality Control (QC) Samples, preferably are por- 6.2 Addition of Oxygen — Place the sample cup in posi-
tions of one or more liquid petroleum materials that are tion and arrange the cotton wisp or nylon thread so that
422
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the end dips into the sample. Assemble the bomb and glass and continue boiling slowly until the solution has
tighten the cover securely. (Warning — Do not add oxygen evaporated to a volume approximately 75 mL as indicated
or ignite the sample if the bomb has been jarred, dropped, by a mark on the beaker. Remove the beaker from the hot
or tilted.) Admit oxygen slowly (to avoid blowing the oil plate (or other source of heat) and allow it to cool for 1
from the cup) until a pressure is reached as indicated in hr before filtering. Filter the supernatant liquid through
the following table: an ashless, quantitative filter paper (Note 5). Wash the
Capacity of Minimum Gage Maximum Gage precipitate with water, first by decantation and then on
Bomb, ml Pressure,A kgf/cm2 (atm) Pressure,A kgf/cm2 (atm) the filter, until free from chloride. Transfer the paper and
300 to 350 39 (38) 41 (40) precipitate to a weighed crucible and dry (Note 6) at a low
350 to 400 36 (35) 38 (37) heat until the moisture has evaporated. Char the paper
400 to 450 31 (30) 33 (32) completely without igniting it, and finally ignite at a bright
450 to 500 28 (27) 30 (29) red heat until the residue is white in color. After ignition
A
The minimum pressures are specified to provide sufficient oxygen for
is complete, allow the crucible to cool at room temperature,
complete combustion and the maximum pressures represent a safety and weigh.
requirement.
NOTE 5 — A weighed porcelain filter crucible (Selas type) of 5 to 9-
6.3 Combustion — Immerse the bomb in a cold distilled- m porosity may be used in place of the filter paper. In this case the
water bath. Connect the terminals to the open electrical precipitate is washed free of chloride and then dried to constant weight
at 500 ±25°C.
circuit. Close the circuit to ignite the sample. (Warning —
Do not go near the bomb until at least 20 s after firing.) NOTE 6 — A satisfactory means of drying, charring, and igniting the
paper and precipitate is to place the crucible containing the wet filter
Remove the bomb from the bath after immersion for at paper in a cold electric muffle furnace and to turn on the current. Drying,
least 10 min. Release the pressure at a slow, uniform rate charring, and ignition usually will occur at the desired rate.
such that the operation requires not less than 1 min. Open
the bomb and examine the contents. If traces of unburned 6.6 Blank — Make a blank determination whenever new
oil or sooty deposits are found, discard the determination reagents, white oil, or other low-sulfur combustible mate-
and thoroughly clean the bomb before again putting it in rial are used. When running a blank on white oil, use 0.3
use (Note 2). to 0.4 g and follow the normal procedure.
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423
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ARTICLE 24, SD-129 2007 SECTION V
9.1.2 Reproducibility — The difference between two where x is the mean of duplicate test results.
single and independent results obtained by different opera- (b) These precision values were obtained in 1960 by statistical exami-
nation of interlaboratory test results. No limits have been established for
tors working in different laboratories on identical test mate- additive concentrates.
rial would, in the long run, in the normal and correct
operation of the test method, exceed the following values 9.2 Bias — Results obtained in one laboratory by Test
only in one case in twenty: Method D 129 on NIST Standard Reference Material Nos.
Sulfur, 1620A, 1621C, and 1662B were found to be 0.05 mass %
Weight % Repeatability Reproducibility higher than the accepted reference values.
0.1 to 0.5 0.04 0.05
0.5 to 1.0 0.06 0.09
1.0 to 1.5 0.08 0.15 10. Quality Control
1.5 to 2.0 0.12 0.25
2.0 to 5.0 0.18 0.27 10.1 Confirm the performance of the instrument or the
test procedure by analyzing a QC sample (see 6.9).
NOTE 7 — The precision shown in the above table does not apply to 10.1.1 When QC/Quality Assurance (QA) protocols
samples containing over 2% chlorine because an added restriction on the
amount of sample which can be ignited is imposed.
are already established in the testing facility, these may be
used to confirm the reliability of the test result.
NOTE 8 — This test method has been cooperatively tested only in the
range of 0.1 to 5.0% sulfur.
10.1.2 When there is no QC/QA protocol established
in the testing facility, Appendix X1 can be used as the
NOTE 9 — The following information on the precision of this method QC/QA system.
has been developed by the Institute of Petroleum (London):
(a) Results of duplicate tests should not differ by more than the follow-
ing amounts:
Repeatability Reproducibility 11. Keywords
0.016 x + 0.06 0.037 x + 0.13 11.1 bomb; sulfur
424
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APPENDIX
(Nonmandatory Information)
X1. QUALITY CONTROL on the criticality of the quality being measured, the demon-
strated stability of the testing process, and customer
X1.1 Confirm the performance of the instrument or the
requirements. Generally, a QC sample is analyzed each
test procedure by analyzing a quality control (QC) sample.
testing day with routine samples. The QC frequency should
X1.2 Prior to monitoring the measurement process, the be increased if a large number of samples are routinely
user of the test method needs to determine the average analyzed. However, when it is demonstrated that the testing
is under statistical control, the QC testing frequency may
value and control limits of the QC sample (see Practice D
be reduced. The QC sample precision should be checked
6299 and MNL 7).
against the ASTM method precision to ensure data quality.
X1.3 Record the QC results and analyze by control X1.5 It is recommended that, if possible, the type of
charts or other statistically equivalent techniques to ascer- QC sample that is regularly tested be representative of the
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tain the statistical control status of the total testing process material routinely analyzed. An ample supply of QC sam-
(see Practice D 6299 and MNL 7). Any out-of-control data ple material should be available for the intended period
should trigger investigation for root cause(s). of use, and must be homogenous and stable under the
anticipated storage conditions. See Practice D 6299 and
X1.4 In the absence of explicit requirements given in MNL 7 for further guidance on QC and control charting
the test method, the frequency of QC testing is dependent techniques.
425
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No reproduction or networking permitted without license from IHS Not for Resale, 11/12/2007 23:43:55 MST